Detection and quantification of milk adulteration using time domain nuclear magnetic resonance (TD-NMR)

Abstract This study explores the possibilities for application of 1H Time Domain Nuclear Magnetic Resonance (1H TD-NMR) as a rapid method for assessment of milk quality. Whey, urea, hydrogen peroxide, synthetic urine and synthetic milk were added to the milk samples at concentrations of 5, 15, 25, 35 and 50% v/v. Discrete exponential analysis of the 1H TD-NMR relaxation decay revealed that the milk samples contained a single water component as well as that the T2 relaxation times differed significantly with respect to the level of adulteration. Regression models obtained with the full 1H TD-NMR (multivariate approach) and T2 value (univariate approach) demonstrate a strong correlation to estimate the level of adulteration in milk samples, with standard errors of prediction of 2.34 and 3.79% v/v, respectively. SIMCA and kNN classification models were developed to classify control from adulterated milk samples and adulterated milk samples based on the level of adulteration. The results obtained with both models showed a similar and quite satisfactorily predictability, with sensitivity and specificity ranging from 0.66 to 1.00. This study clearly demonstrates that 1H TD-NMR could be applied as an alternative rapid method for detecting and quantifying milk adulteration.

[1]  Eliane Teixeira Mársico,et al.  Classification of Brazilian honeys by physical and chemical analytical methods and low field nuclear magnetic resonance (LF 1H NMR) , 2014 .

[2]  H. J. Andersen,et al.  Comparative study of low-field NMR relaxation measurements and two traditional methods in the determination of water holding capacity of pork. , 2001, Meat science.

[3]  Carmen Rosselló,et al.  Validation of a Difussion Model Using Moisture Profiles Measured by Means of TD-NMR in Apples (Malus domestica) , 2013, Food and Bioprocess Technology.

[4]  F. Mariette,et al.  Evolution of water proton nuclear magnetic relaxation during milk coagulation and syneresis: Structural implications , 1993 .

[5]  L. Rodriguez-Saona,et al.  Application of hand-held and portable infrared spectrometers in bovine milk analysis. , 2013, Journal of agricultural and food chemistry.

[6]  Yi-Qiao Song A 2D NMR method to characterize granular structure of dairy products , 2009 .

[7]  Hanne Christine Bertram,et al.  Relationship between meat structure, water mobility, and distribution: a low-field nuclear magnetic resonance study. , 2002, Journal of agricultural and food chemistry.

[8]  F. Capozzi,et al.  Influence of the season on the relationships between NMR transverse relaxation data and water-holding capacity of turkey breast meat , 2004 .

[9]  H. J. Andersen,et al.  Direct decomposition of NMR relaxation profiles and prediction of sensory attributes of potato samples , 2003 .

[10]  H. van As,et al.  Time domain NMR applied to food products , 2010 .

[11]  Edenir Rodrigues Pereira-Filho,et al.  Digital image analysis - an alternative tool for monitoring milk authenticity , 2013 .

[12]  J. Spink,et al.  Development and application of a database of food ingredient fraud and economically motivated adulteration from 1980 to 2010. , 2012, Journal of food science.

[13]  Eliane Teixeira Mársico,et al.  Detection of honey adulteration of high fructose corn syrup by Low Field Nuclear Magnetic Resonance (LF 1H NMR) , 2014 .

[14]  J. Braga,et al.  Development and validation of a chemometric method for direct determination of hydrochlorothiazide in pharmaceutical samples by diffuse reflectance near infrared spectroscopy , 2013 .

[15]  S. Engelsen,et al.  NMR-cooking: monitoring the changes in meat during cooking by low-field 1H-NMR , 2002 .

[16]  Fabíola Manhas Verbi Pereira,et al.  Through-package fat determination in commercial samples of mayonnaise and salad dressing using time-domain nuclear magnetic resonance spectroscopy and chemometrics , 2015 .

[17]  Pervez Mustajab,et al.  Determining the adulteration of natural milk with synthetic milk using ac conductance measurement , 2006 .

[18]  H. J. Andersen,et al.  Water distribution and mobility in meat during the conversion of muscle to meat and ageing and the impacts on fresh meat quality attributes--a review. , 2011, Meat science.

[19]  Yi-Qiao Song,et al.  Quantitative characterization of food products by two-dimensional D-T2 and T1-T2 distribution functions in a static gradient. , 2006, Journal of colloid and interface science.

[20]  J. Koenderink Q… , 2014, Les noms officiels des communes de Wallonie, de Bruxelles-Capitale et de la communaute germanophone.

[21]  José Bon,et al.  Moisture profiles in cheese drying determined by TD-NMR: Mathematical modeling of mass transfer , 2011 .

[22]  Mercedes Careche,et al.  Estimation of freezing storage time and quality changes in hake (Merluccius merluccius, L.) by low field NMR. , 2012, Food chemistry.

[23]  Q. Shen,et al.  Discrimination of Edible Vegetable Oil Adulteration with Used Frying Oil by Low Field Nuclear Magnetic Resonance , 2013, Food and Bioprocess Technology.

[24]  Miss A.O. Penney (b) , 1974, The New Yale Book of Quotations.

[25]  M. Sena,et al.  Use of NIRS to predict composition and bioethanol yield from cell wall structural components of sweet sorghum biomass , 2014 .

[26]  Henrik Toft Pedersen,et al.  Low-field 1H nuclear magnetic resonance and chemometrics combined for simultaneous determination of water, oil, and protein contents in oilseeds , 2000 .

[27]  Richard Ipsen,et al.  Water mobility in acidified milk drinks studied by low-field 1H NMR , 2007 .

[28]  Fabíola Manhas Verbi Pereira,et al.  Classification of intact fresh plums according to sweetness using time-domain nuclear magnetic resonance and chemometrics , 2013 .

[29]  A. Hesse,et al.  Laser-probe-based investigation of the evolution of particle size distributions of calcium oxalate particles formed in artificial urines , 2001 .